1. Grant Mills SPB/SFX Postdoctoral Scientist Hamburg DESY, 09 June 2017
Seeing elusive protein structures at high resolution: Instrumentation for XFEL crystallography and imaging
Grant Mills
SPB/SFX
Postdoctoral Scientist
Hamburg DESY, 09 June 2017

2. The European XFEL

3. Traditional X-ray sources
Images:

4. Protein structure Nass et al. (2016) TRM Barends et al. (2014)
R Neutze (‎2015)

5. Scattered x-rays is proportional to N2 (~ 100 x 100 x 100 elements)
Non-crystalline material scatters fewer x-rays than crystalline material
Scattered x-rays is proportional to N2
(~ 100 x 100 x 100 elements)
If N=1, then scattering is proportional to 1
(~ a million times less than above)
Conclusion: Need a lot more x-rays
Slide modified: A. P. Mancuso

6. SASE radiation
FELs offer improvements over 3rd generation synchrotrons
Orders of magnitude brighter
Extremely short pulse duration
Both µm and nm focus

7. Diffraction before destruction
Image: R. Neutze et al. Nature (2000)

8. SASE pulse train
Slide: A. P. Mancuso

9. Undulator

10. Undulator

11. Undulator Coherent radiation is emitted from 175 m of SASE undulator
Initial section of undulator produces radiation
The radiation couples with the electron’s to bunch the electrons
Saturation occurs when the electrons are completely microbunched
This process greatly amplifies the radiation emitted

12. Radiation damage Diffraction before destruction (2014)
Henry N. Chapman, Carl Caleman, Nicusor Timneanu

13. Imaging biomolecules and X-ray radiation
Technical Design Report: Scientific Instrument SPB, (2013) A. P. Mancuso, et al.

14. KB mirror systems
Kirkpatrick-Baez mirrors will produce a 1 micron and 100 nanometer focused beam
4 bounce system (1 µm) in green
2 bounce system (100 nm) in blue
B4C and Ru coatings
Design of the mirror optical systems for coherent diffractive imaging at the SPB/SFX instrument of the European XFEL, (2016) Richard J Bean, et al.

15. KB mirror systems
Kirkpatrick-Baez mirrors will produce a 1 micron and 100 nanometer focused beam
4 bounce system (1 µm) in green
2 bounce system (100 nm) in blue
B4C and Ru coatings
Design of the mirror optical systems for coherent diffractive imaging at the SPB/SFX instrument of the European XFEL, (2016) Richard J Bean, et al.

16. KB mirror systems micron focus nano focus
Design of the mirror optical systems for coherent diffractive imaging at the SPB/SFX instrument of the European XFEL, (2016) Richard J Bean, et al.

17. Manufacturing achievements
970 x 25 mm clear aperture
1.8 nm peak to valley variation
2x 50 nm thick polished coatings
B4C and Ru
950 x 10 mm

18. Compound refractive lenses
Initial operation will use the CRL in the tunnel
CRL is a repeating structure of parabolic surfaces
12 mm diameter
2 mm thickness
Focus to 2.5 µm diameter
Refractive x-ray lenses (2005) B. Lengeler, et al

19. Cassette ordering Initial operation will use the CRL in the tunnel
1, 2, 4, 8, 10, 10 …..
Allows the change of X-ray energy while still maintaining focal location

20. Interaction region
There are two inline interaction regions, thes 1st upstream region is available day 1
Day 1 will provide 60 pulses per train at 10 Hz
Photons at 8.4 keV
Pulse energy at 2 mJ
Pulse duration 43 fs
120° open scattering cone
Image: Joachim Schulz

21. Sample injection
Many methods have been adopted to deliver sample into the interaction region
GDVN
Aerosol
Fixed targets
Images: J. Schulz and R. Graceffa

22. Gas Dynamic Virtual Nozzle
Capillary guides the sample into the interaction region
Inert gas focuses the jet into a thin stream
A µm thin jet can be maintained over more than 100 µm distance
A modified system can also handle viscous solutions
Image:

23. Design study of a microfluidic mixing nozzle in 25 mm nozzle rod
Image: Joachim Schulz, Rita Graceffa, Dennis Ropers

24. Aerosol injectors Injector creates particle beam
Pressures decrease through the injector nozzle
Rapid motion of sample
Image: Joachim Schulz

25. Fixed targets
Image: Joachim Schulz

26. AGIPD Detectors 6 – 13 keV 1 x 104 at 12 keV dynamic range
5 σ at 12 keV sensitivity
Number of storage cells 352
Can store images at 4.5 MHz
Image: AGIPD Consortium

27. Experiments
Slide modified: Adam Round

28. The Single Particle Imaging Experiment
Image: Gaffney, Champman. Science (2007)

29. Experiments Time-resolved SFX Bacteriorhodopsin conformational changes
10 fs long pulses at SACLA
Eriko Nango, et al 2017, Science

30. Experiments High resolution SFX 1.2 Å res proteinase K
Comparision of SFX and SRX B-factors
Tetsuya Masuda, et al 2017, Science Reports

31. Experiments
Two-colour X-ray-pump/X-ray-probe scheme used for studying the molecular fragmentation of XeF2
These reactions occur on the fs timescale, perfect for the European XFEL
A Picón, et al 2016
CS Lehmann, et al 2016

32. Experiments

33. Acknowledgments: People—the most important components
Sample Environment
AGIPD consortium
Adrian Mancuso
Zunaira Ansari
Richard Bean
Johan Bielecki
Carsten Fortmann-Grote
Klaus Giewekemeyer
Oliver Kelsey
Felix Lemcke
Luis Lopez Morillo
Bradley Manning
Masoud Mehrjoo
Marc Messerschmidt
Nadja Reimers
Adam Round
Tokushi Sato
Marcin Sikorski
Andrew Stawniczy
Stephan Stern
Britta Weinhausen
Patrik Vagovic
Prasad Thute
Particular thanks to all European XFEL groups supporting (too many to mention).